Identification of barbiturates by chemical ionization and mass-analyzed ion kinetic energy spectrometry

Soltero-Rigau, E.; Kruger, T. L.; Cooks, R. Graham

doi:10.1021/ac50011a027

Cited by 35 publications

(8 citation statements)

References 47 publications

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“…resulting from the c.i.d. ofisomeric ion structures have been shown to be capable of easily distinguishing between them [20][21][22]. We have previously reported the combination of these techniques to identify unambiguously cyclic AMP, cyclic GMP and cyclic CMP as distinct from their 2',3'-cyclic isomers in tissue extracts [3,23,24], and we have now extended this approach so that the unequivocal identification of microgram quantities of 3',5'-cyclic UMP, -cyclic IMP, -cyclic XMP and -cyclic dTMP is possible [25].…”

Section: Introductionmentioning

confidence: 99%

Extraction, purification, identification and metabolism of 3′,5′-cyclic UMP, 3′,5′-cyclic IMP and 3′,5′-cyclic dTMP from rat tissues

Newton¹,

Kingston²,

Hakeem³

et al. 1986

Biochemical Journal

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The large-scale extraction and partial purification of endogenous 3',5'-cyclic UMP, 3',5'-cyclic IMP and 3',5'-cyclic dTMP are described. Rat liver, kidney, heart, spleen and lung tissues were subjected to a sequential purification procedure involving freeze-clamping, perchlorate extraction, alumina and Sephadex ion-exchange chromatography and preparative electrophoresis. The samples thus obtained co-chromatographed with authentic cyclic UMP, cyclic IMP and cyclic dTMP on t.l.c. and h.p.l.c. and the u.v. spectra of the extracted samples were identical with those of the standards. Fast atom bombardment of the three cyclic nucleotide standards yielded mass spectra containing a molecular protonated ion in each case; mass-analysed ion kinetic-energy spectrometry ('m.i.k.e.s') of these ions produced a spectrum unique to the parent cyclic nucleotide. The extracted putative cyclic UMP, cyclic IMP and cyclic dTMP each produced a m.i.k.e.s. identical with that obtained with the corresponding cyclic nucleotide standard. Rat liver, heart, kidney, brain, intestine, spleen, testis and lung protein preparations were each found capable of the synthesis of cyclic UMP, cyclic IMP and cyclic dTMP from the corresponding nucleoside triphosphate, of the hydrolysis of these cyclic nucleotides and of their binding, with the exception that cyclic dTMP was not synthesized by the kidney preparation.

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Section: Introductionmentioning

confidence: 99%

Extraction, purification, identification and metabolism of 3′,5′-cyclic UMP, 3′,5′-cyclic IMP and 3′,5′-cyclic dTMP from rat tissues

Newton¹,

Kingston²,

Hakeem³

et al. 1986

Biochemical Journal

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“…Recently, Harvan^(412) discussed, and compared, the electron impact (El), methane-positive chemical ionization (MPCI), oxygen-negative chemical ionization (ONCI), and collision-induced dissociation, mass-analyzed, ion kinetic energy (CID-MIKE) spectra (208,414,425,426) of the nine metabolites of DEHP isolated from rat urine. The metabolites were methylated with diazomethane, and fractions were purified by LC on a Porasil A-60 column using a tetrahydrofuran -hexane gradient (prefractionation is necessary).…”

Section: Recent Lc-ms Methodsmentioning

confidence: 99%

Priority toxic pollutants in human urine :

Fatiadi¹

1983

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“…MS/MS as an analytical technique was still in its infancy, with the research groups of Cooks and McLafferty at the forefront of the development [1][2][3][4][5][6][7][8][9][10][11][12]. For all this early work, sector instruments were used exclusively and CID was performed at high kinetic energies.…”

Section: Beam-beam Hybrid Instrumentsmentioning

confidence: 99%

Hybrid mass spectrometers for tandem mass spectrometry

Glish

Burinsky

2008

J. Am. Soc. Mass Spectrom.

101

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Mass spectrometers that use different types of analyzers for the first and second stages of mass analysis in tandem mass spectrometry (MS/MS) experiments are often referred to as "hybrid" mass spectrometers. The general goal in the design of a hybrid instrument is to combine different performance characteristics offered by various types of analyzers into one mass spectrometer. These performance characteristics may include mass resolving power, the ion kinetic energy for collision-induced dissociation, and speed of analysis. This paper provides a review of the development of hybrid instruments over the last 30 years for analytical applications. (J Am Soc Mass Spectrom 2008, 19, 161-172) © 2008 American Society for Mass Spectrometry T andem mass spectrometry (MS/MS), in a very generic description, is a process in which an ion formed in an ion source is mass-selected in the first stage of analysis, reacted, and then the charged products from the reaction are analyzed in the second stage of analysis. The type and quality of data that is obtained can vary greatly depending upon the type of analyzer used in the first and second stages of analysis, and the type of reaction performed between the stages of analysis. The reactions that can be done also can depend upon the type of analyzer. Over the years there have been a variety of means developed to measure the mass-to-charge ratio of gas-phase ions. The most common methods involve: dispersion based on ion momentum or kinetic energy (magnetic and electric sector instruments); separation in time based on ion velocity (time-of-flight); transmission through an electrodynamic field (quadrupole mass filter); and periodic motion in a magnetic or electrodynamic field (ion traps). There are differences in the experimental parameters associated with these various analysis methods that are pertinent to the MS/MS experiment. Some parameters are obvious, typically related to the performance of the mass analyzer while others are more subtle, related to the reactions/chemistry occurring between the stages of analysis. Many times these different parameters are used to categorize MS/MS experiments.One parameter is the ion kinetic energy. Sector and time-of-flight (TOF) instruments typically operate at "high" ion kinetic energies (5-20 keV), whereas "low" ion kinetic energies (Ͻ50 eV) are typical in quadrupole mass filters and ion traps. The ion kinetic energy is an important parameter in MS/MS experiments because the most common reaction involves colliding the ion of interest with a target gas atom or molecule. When performing ion-neutral collision experiments, the possible reactions that can be accessed (e.g., collisioninduced dissociation, collisional cooling, charge permutation, ion/molecule reaction) depends upon the ion kinetic energy. The appearance of the MS/MS spectrum can change drastically as a function of the collision (ion kinetic) energy. A related factor that is equally important, but often not considered, is the time frame of the experiment, that is, the elapsed time bet...

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Identification of barbiturates by chemical ionization and mass-analyzed ion kinetic energy spectrometry

Cited by 35 publications

References 47 publications

Extraction, purification, identification and metabolism of 3′,5′-cyclic UMP, 3′,5′-cyclic IMP and 3′,5′-cyclic dTMP from rat tissues

Extraction, purification, identification and metabolism of 3′,5′-cyclic UMP, 3′,5′-cyclic IMP and 3′,5′-cyclic dTMP from rat tissues

Priority toxic pollutants in human urine :

Hybrid mass spectrometers for tandem mass spectrometry

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